反应详情

A solution of 2,4′-dichlorobenzhydrol (7) (178 mmol), p-toluenesulphonic acid (198 mmol) and 1-benzhydryl-3-azetidinol (1) (99 mmol) in toluene (500 mL) was heated at reflux in a Dean-Stark apparatus for 40 minutes. The solution was cooled, washed with sodium hydrogen carbonate (saturated aqueous solution, 700 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography [SiO2; (10% ethyl acetate:isohexane)] to finish the product as a yellow oil (17.8 g, 38%).

1. temperatureat reflux in a Dean-Stark apparatus for 40 minutes
2. temperatureThe solution was cooled
3. washwashed with sodium hydrogen carbonate (saturated aqueous solution, 700 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography [SiO2; (10% ethyl acetate:isohexane)]